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Production of multi-wall carbon nanotubes starting from a commercial

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Article in FME Transactions · January 2018

DOI: 10.5937/fmet1802151K

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 Claudir Gabriel Kaufmann Jr
Researcher
Federal University of Rio Grande do Sul
Production of Multi-wall Carbon
Brazil
Nanotubes Starting from a Commercial
Rúbia Young Sun Zampiva Graphite Pencil using an Electric Arc
Researcher
Federal University of Rio Grande do Sul
Brazil
Discharge in Aqueous Medium
Carlos Pérez Bergmann Carbon nanotubes (CNTs) are studied because of their diverse
Professor applications in many fields, such as medicine, computing, physics,
Federal University of Rio Grande do Sul chemistry, and others. Therefore, it is crucial to develop techniques for
Brazil
producing a large volume of high-quality multi-wall carbon nanotubes
Annelise Kopp Alves (MWCNTs) with the best cost-to-benefit ratio. In this paper, we obtain
Professor MWCNTs via an arc-electric alternative route, which dispenses catalysts
Federal University of Rio Grande do Sul and sealed cameras using water as an insulating medium. This method is
Brazil simple, cost-effective (starting from pieces of commercial graphite pencil),
Sergio Roberto Mortari efficient, and highly reproducible. Since no catalysts are used, no
purification post-treatment was necessary, leading to high-quality
Professor
Franciscan University Center MWCNTs. This technique is very promising for industrial applications
Brazil because a lot of high-quality MWCNTs could be easily produced in a short
time.
Ana Pavlovic
Reseacher
University of Bologna Keywords: Synthesis of MWCNT, electric arc discharge, commercial
Italy graphite pencil.

1. INTRODUCTION

Nanotechnology has been the focus of research in

several fields becoming a real revolution in science and
technology. It is commercially used in products such as
cosmetics, chips and building materials. As a definition,
nanotechnology is understood as the manipulation of
nanoscale structures in the order of atomic and
molecular size. The nanoscale is defined as the billionth
part of the meter (10-9m) [1]. The manipulation in this
order of magnitude has awakened a series of studies in
the areas of health, computing, physics, chemistry,
materials, among others. The primary motivation of
research in nanotechnology is the development of new
materials with specific properties that will improve the
materials and substances existing in the micrometric and
macrometric scale (as in [2, 3]). Theoretical and
experimental studies of synthesis, purification, and
characterization of nanostructures have been enhanced
since these new nanomaterials do not always meet all
the necessary specifications (mainly the degree of
purity) for commercial applications [4-6]. Carbon
nanotubes (CNTs) are structures formed by flat sheets Figure 1. Schematic representation of a) a graphene sheet
and b) a single wall CNT. Adapted from larrude, 2007 [7,8].
of graphene that, at a particular temperature, become
rolled into tubes with a nanometer-scale diameter [7, 8]. The carbon atoms in the SWCNTs form a hexagonal
Depending on the synthesis method, it is possible to network, consisting of single and double bonds with sp2
obtain single wall CNTs (SWCNTs), double wall CNTs hybridization. The MWCNTs (Figure 2) are formed by
(DWCNTs) and multiple walls (MWCNTs). The several SWCNTs in a coaxial-like structure. (Larrudé,
SWCNT is formed by a single coiled graphite layer (a 2007). CNTs have, in general, less than 100 nm in
graphene sheet), which may have its ends closed by diameter and several micrometers in length. CNTs have
halves of fullerenes or open, as represented in Figure 1. a defined crystalline structure, as well as physical pro–
perties characteristics of oriented crystals, such as high
Received: March 2017, Accepted: October 2017 conductivity and mechanical resistance [8-10].
Correspondence to: Dr Claudir Gabriel Kaufmann Jr CNTs also present different chiralities depending on
Federal University of Rio Grande do Sul - UFRGS. the synthesis method. They can show three different
Osvaldo Aranha 99, Porto Alegre, RS 90035- 190, BR. orientation; Armchair, ZigZag, and Chiral. The arm–
E-mail: gabrielklpgodines@gmail.com chair CNTs have a metallic behavior, while the two
doi: 10.5937/fmet1802151K
© Faculty of Mechanical Engineering, Belgrade. All rights reserved FME Transactions (2018) 46, 151-156 151
others are semi metallic. The manipulation of CNTs has
resulted in a series of studies in the areas of health,
computing, physics, chemistry, and materials.
Figure 2. Schematic representation of a SWCNT and an
MWCNT [11].
To produce CNTs, the most common methods are:
chemical vapor deposition (CVD) [12], combustion
[13], laser ablation [14], and electric arc [15, 16]. The
CVD method produces CNTs based on the deposition of
carbon precursor gases, while the combustion method is
based on the combustion of carbon precursor gases. The
production of CNTs by laser ablation and electric arc
methods come from the sublimation of carbon atoms
from a solid precursor, often mineral graphite. The
electric arc method consists of an electric discharge
generated by two carbon electrodes in a steel chamber
containing an inert gas (usually helium) [17,18,19]. The
electrodes (cathode and anode) are kept at a relatively
short distance from each other (about 1 mm), generating
plasma between them. The plasma temperature between
the electrodes is extremely high (3000-4000°C) [20].
The precursor is sublimated at the positive electrode
(anode), and the nanomaterials that form are deposited
at the negative electrode (cathode) and on the chamber
walls. The electric arc method in an aqueous medium is
a variation of the conventional electric arc method. This
process is simpler because it dispenses with the need for
a sealed chamber, vacuum, and gas flow [21]. Water
acts as an insulating medium and keeps the system cool.
Over the years, several theoretical and experimental
studies of CNT synthesis and purification have been
conducted. Most of these synthesis techniques do not
achieve the minimum standards, especially concerning
nanostructure purity [22–25]. Most of these methods
(CVD, Combustion, HiPco, and others) use metal
catalysts, leading to post-synthesis purification
processes [26, 27]. These methods increase the
production costs, and because of the use of strong acids,
they directly affect the CNT structure, resulting in high
rates of defective CNT products [28]. In this paper, we
describe the production of MWCNTs using the electric
152 ▪ VOL. 46, No 2, 2018
arc technique in an aqueous medium. Commercial grap–
hite pencils were used as a carbon precursor, which
dispensed with the need for catalysts.
2. MATERIALS AND METHODS
2.1 Synthesis of MWCNTs
The reactor used in this work is divided into three parts:
Mechanical; Electrical and Software. The mechanical
part is understood by the support structures, tongs, and
motors. The electronics are composed of a controller
interface (control board). The software part has the
responsibility of managing the system. A picture of the
arc electric discharge system indicating all the com–
ponents is presented in Figure 3.
Figure 3. Picture of the arc electric discharge system. The
numbers identify the components described in the text.
The numbers in Figure 3 indicate the components of
the electric arc reactor used in this work for the
MWCNTs production, where: (1) Stepper motor used to
rotate the anode electrode (left electrode); (2) Tweezers
for attaching graphite electrodes; (3) Acrylic tank (water
tank); (4) Iron support used to support the other parts of
the reactor; (5) Stem where the cathode electrode (right
electrode) slides approaching the anode electrode
(which is fixed); (6) Power supply of the control board;
(7) Control board, which manages the system; (8)
Electric source of alternating current for the formation
of plasma (soldering machine).
Figure 4a shows, schematically, the MWCNT
synthesis by an electric arc discharge in aqueous
medium proposed in this work. A commercial graphite
pencil (6B) from Faber-Castell was used as carbon
precursor (Figure 4b).
According to previous thermogravimetric analyses,
these graphite pencils are composed of 51% graphite
and 49% amorphous carbon and polymeric structures.
The plastic around the graphite pencils was
removed. The exposed graphite (95 mm long, 8 mm in
diameter, and 8 g) was fixed to the cathode and anode.
The system was submerged in Milli-Q water (18.2
μS/cm) while avoiding interaction with the atmosphere.
A continuous current of 80 A was applied while the cat–
hode and anode were slowly separated to a distance of
approximately 1 mm. At this point, the applied current
generated plasma (Figure 4c) between the electrodes,
reaching temperatures of around 3000-4000°C. This led
to sublimation of the carbon precursor (anode). The
cathode was not affected during this process. The
synthesis took around 5 min.
FME Transactions

Figure 4. a) Scheme of MWCNT synthesis using an electric
arc discharge in an aqueous medium. b) Image of the 6B
graphite pencils used as a carbon precursor and c) the
plasma generated at 80 A.
The product was vacuum filtered to separate it from
the water and then thermally treated at 500°C to remove
amorphous carbon. These processes took about 40 min.
The complete MWCNT synthesis took 45 min.
2.2 Chemical and structural characterization
The sample was analyzed by Raman spectroscopy in a
Renishaw inVia Spectrometer at 25 °C, in a range of 0
to 2500 cm-1 with a 532 nm laser. The Raman spectro–
scopy was preferred respect to other methods (as
infrared [29, 30]) since its large application on graphite.
The morphology was characterized by scanning electron
microscopy (SEM) in a JEOL microscope (JSM 6060)
FME Transactions
with a maximum operational tension of 30kV and a
nominal resolution of 3.5 nm. The applied tension was
10 to 20 kV.
Transmission electron microscopy (TEM) was per–
formed on a JEOL microscope (JEM 1200 EXII model).
This equipment operates between 80kV and 100kV,
with a punctual resolution of 0.45 nm and line reso–
lution of 0.2 nm. The magnification range was from
5,000x to 500,000x.
3. RESULTS
The Raman spectrum revealed the MWCNT charac–
teristics of the D, G, and G' bands at 1,342 cm-1, 1,572
cm-1, and 2,738 cm-1, respectively [31, 32] (Figure 5).
The G' band indicates the degree of purity for the
MWCNTs. The higher the G' band intensity compared
to the D and G bands, the higher the MWCNT purity,
which translated to less amorphous carbon and defects
[31]. MWCNT quality and quantity were also measured
using the (ID/IG) ratio. This ratio is related to the carbon
graphitization degree [33]. The lower the ratio, the
higher the graphitization degree and the higher the
quality and quantity of CNTs present in the sample [32].
The MWCNTs we synthesized had a ratio of 0.243
ID/IG, indicating an elevated graphitization degree and,
consequently, the formation of high-quality CNTs [24].
Next, 2 g of MWCNTs were produced using the
synthesis method we developed, resulting in about 25%
of the production yield. The MWCNTs displayed high
quality with just a few structural defects (Figures 6 and
7). The yield was calculated based on the mass balance.
The anode electrode (carbon precursor) had a mass of 8
g, around 51% of the precursor was graphite (about 4 g),
and the remainder was composed of structure-sustaining
polymers and amorphous carbon. For the production of
CNTs using the electric arc, only the pure graphite
portion was used [34]. Graphite has high conductivity,
facilitating the sublimation of the carbon atoms [35].
Electrodes with high conductivity generate higher tem–
peratures in the plasma, leading to elevated carbon
sublimation rates.
Figure 5. Raman spectrum of the synthesized MWCNTs.
The higher the quantity of sublimated atoms, the
greater the quantity and quality of the MWCNTs
produced. Polymeric amorphous and/or carbonaceous
VOL. 46, No 2, 2018 ▪ 153
structures exhibit low conductivity, which hampers the
sublimation of carbon [35]. It is, therefore, possible that
only about 51% of the pencil was ultimately used in the
MWCNT synthesis. Although about 50% of this pre–
cursor can be used, the cost-benefit ratio is still high
concerning mineral graphite precursors (99% purity)
because these have a high cost (about one hundred times
more expensive than the method described here) [36].
Figure 6. SEM image of the synthesized MWCNTs.
Figure 7. a) TEM images of MWCNTs. b) HRTEM of a single
MWCNT with an internal diameter of 18.70 nm and an
external diameter of 68.17 nm.
The 25% production yield is considered satisfactory
when compared to other production techniques [26, 27].
With the exception of chemical vapor deposition
(CVD), the other existing techniques take much more
hours to produce the same quantity of MWCNTs (2 g).
154 ▪ VOL. 46, No 2, 2018
The method we developed takes 45 min. Besides, this
synthesis technique does not require the use of catalysts,
which are indispensable for CVD methods. A fast syn–
thesis approach, which skips MWCNT purification
stages, is very industrially feasible. It is possible to pro–
duce large quantities of MWCNTs of high quality, avo–
iding structural defects related to acid purification
treatments [22, 23].
The TEM image (Figure 7a) shows some MWCNTs
with an average internal diameter of 10 nm and an
average external diameter of 30 nm. The HRTEM
(Figure 7b) proved the existence of an MWCNT, which
had an internal diameter of 18.70 nm and an external
diameter of 68.17 nm. The nanotube structure was
formed by more than 40 tubular walls.
The CNT sponge-like structure was composed of
disorganized, tangled MWCNTs (Figure 7b). The
MWCNTs had diameters ranging from 10-100 nm and
lengths of approximately 10 µm.
4. CONCLUSIONS
The proposed synthesis method was effective for gene–
rating mwcnts, and we successfully generated a large
quantity of high-quality mwcnts. Also, this technique
dispenses with purification treatments, as well as the use of
catalysts. The system that applied the electric arc in aqu–
eous medium did not require expensive furnaces, lasers, or
vacuum chambers, considerably reducing the processing
costs. The use of commercial pencils as precursors
suggests that we can produce high-quality mwcnts while
recycling discarded materials. Cumula–tively, the data
presented in this paper makes this approach a useful, low-
cost, large-scale technique for producing high-quality
mwcnts in an environmentally conscious fashion.
ACKNOWLEDGMENTS
The authors would like to thank the Coordination for the
Improvement of Higher Education Personnel- CAPES
for the financial support and the Center of Microscopy
and Microanalysis of Federal University of Rio Grande
do Sul (CMM/UFRGS) for the technical support.
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ПРОИЗВОДЊА ВИШЕСЛОЈНИХ УГЉЕНИЧ–
НИХ НАНОЦЕВКИ ПОЛАЗЕЋИ ОД КОМЕР–
ЦИЈАЛНИХ ГРАФИТНИХ ОЛОВАКА
156 ▪ VOL. 46, No 2, 2018
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КОРИШЋЕЊЕМ ПРАЖЊЕЊА ЕЛЕКТ–
РИЧНОГ ЛУКА У ВОДЕНОЈ СРЕДИНИ
К. Кауфман, Р. Зампива, К. Бергман, А. Алвес,
С. Мортари, А Павловић
Карбонске наноцеви (CNT) су проучаване због
различитих примена у многим областима, као што су
медицина, рачунарство, физика, хемија и друге. Због
тога је кључно развити технике за производњу
великог броја висококвалитетних вишезидних угље–
ничних наноцеви (MVCNT) са најбољим односом
трошкова и бенефита. У овом раду добијене су
MVCNT-ови коришћењем правца електричног алт–
ернативног лука, који користећи воду као изо–
лациону средину остварује катализу. Овај метод је
једноставан, исплатив (почев од комада комер–
цијалне графитне оловке), ефикасан и високо репро–
дуктибилан. Пошто се не користе катализатори, није
потребан било који додатни третман пречишћа–
вања, што је доводи до високо–квалитетних MVCNT.
Ова техника је веома перспективна за индустријске
примене, јер се за врло кратко време лако може
произвести много висококвалитетних MVCNT.
FME Transactions